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Modified guidelines for geopolymer concrete mix design using Indian

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Article  in  Asian Journal of Civil Engineering · January 2012

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ASIAN JOURNAL OF CIVIL ENGINEERING (BUILDING AND HOUSING) VOL. 13, NO. 3 (2012)
PAGES 353-364

MODIFIED GUIDELINES FOR GEOPOLYMER CONCRETE MIX

DESIGN USING INDIAN STANDARD

R. Anuradha*a, V. Sreevidyaa, R. Venkatasubramania and B.V. Ranganb

a
Department of Civil Engineering, VLB Janakiammal College of Engineering and Technology
Kovaipudur, Coimbatore – 641 042, India
b
Curtin University of Technology, Perth, Australia
Received: 5 January 2011, Accepted: 25 April 2011

ABSTRACT

This experimental study is intended to identify the mix ratios for different grades of
Geopolymer Concrete by trial and error method. A new Design procedure was formulated for
Geopolymer Concrete which was relevant to Indian standard (IS 10262-2009). The
applicability of existing Mix Design was examined with the Geopolymer Concrete. Two kinds
of systems were considered in this study using 100% replacement of cement by ASTM class
F flyash and 100% replacement of sand by M-sand. It was analyzed from the test result that
the Indian standard mix design itself can be used for the Geopolymer Concrete with some
modification.

Keywords: Alumina-silicate; fly ash; geopolymer concrete; M-sand; mix design.

1. INTRODUCTION

Geopolymers are inorganic polymeric materials with a chemical composition similar to zeolites but
possessing an amorphous structure. Geopolymers may be seen as man-made rocks. They can be
produced by reacting solid aluminosilicates with a highly concentrated aqueous alkali hydroxide or
silicate solution. The chemistry and terminology of inorganic polymers was first discussed in detail
by Davidovits [1]. Since the first mention of the term ‘geopolymer’ by Davidovits [1],
Geopolymers form three-dimensional disordered frameworks of the tecto-aluminosilicate type with
the general empirical formula Mn[-(SiO2)z-AlO2]n.wH2O, in which n is the degree of
polycondensation, and M is predominantly a monovalent cation (K+, Na+), although Ca2+ may
replace two monovalent cations in the structure [2].
The present work is carried out in the framework of a project aims to produce the
geopolymeric Mix procedure of different grade of geopolymer concrete matrices, stronger and
denser equal to the cement concrete obtained by using Portland Cement binders, that can be

*
E-mail address of the corresponding author: anuradhastalin@gmail.com (R. Anuradha)
354 R. Anuradha, V. Sreevidya, R. Venkatasubramani and B.V. Rangan

used for the long term stabilization of inorganic toxic waste i.e. flyash. The particular work
presented in this paper deals with a study investigating the Mix design.

2. MATERIALS USED

Cementitious material used in this Experimental programme was low calcium Flyash (ASTM
type F) [2]. The specific gravity Fly Ash was 2.3. The Specific gravity and Fineness modules
for manufactured sand were 3.1 and 2.15 respectively. The chemical composition for
cementitious material is shown in table 3. Locally available crushed granite stone aggregate of
size 20 mm passing and retained in 10 mm, was used and the specific gravity and fineness
modulus for the same are 2.6 and 6.4 as per IS: 2386- 1968 Part III. Both the Aggregates
compiled with the requirements of IS: 383-1970.Specific gravity of NaoH and Na2Sio3
solutions were 1.47 and 1.6 respectively.

2.1 M-SAND
M-sand is crushed aggregates produced from hard granite stone which is cubically shaped
with grounded edges, washed and graded with consistency to be used as a substitute of river
sand. M-Sand is superior quality manufactured sand with international standards [3].

2.2 Sodium hydroxide

Generally the sodium hydroxides are available in solid state by means of pellets and flakes.
The cost of the sodium hydroxide is mainly varied according to the purity of the substance.
Since our geopolymer concrete is homogenous material and its main process to activate the
sodium silicate, so it is recommended to use the lowest cost i.e. up to 94% to 96% purity. In
this investigation the sodium hydroxide pellets were used. Whose physical and chemical
properties are given by the manufacturer is shown in Table 1 and 2.

Table 1: Physical Properties Sodium hydroxide

Colour Colour less

Specific Gravity
20% 1.22
30% 1.33
40% 1.43
50% 1.53

2.3 Sodium silicate

Sodium silicate is also known as water glass or liquid glass, available in liquid (gel) form. In
present investigation sodium silicate 2.0 (ratio between Na2O to SiO2) is used. As per the
manufacture, silicates were supplied to the detergent company and textile industry as bonding
agent. Same sodium silicate is used for the making of geopolymer concrete. The chemical
 MODIFIED GUIDELINES FOR GEOPOLYMER CONCRETE... 355

properties and the physical properties of the silicates are given the manufacture is shown in
Table 3.
Table 2: Chemical properties sodium hydroxide

Assay 97% Min

Carbonate
2% Max
(Na2CO3)
Chloride (Cl) 0.01% Max

Sulphate (SO2) 0.05% Max

Lead (Pb) 0.001% Max
Iron (Fe) 0.001% Max
Potassium (K) 0.1% Max
Zinc (Zn) 0.02% Max

2.4 Alkaline liquid

Generally alkaline liquids are prepared by mixing of the sodium hydroxide solution and
sodium silicate at the room temperature. When the solution mixed together the both solution
start to react i.e. (polymerisation takes place) it liberate large amount of heat so it is
recommended to leave it for about 24 hours thus the alkaline liquid is get ready as binding
agent [4].

2.5 Preparation of alkaline liquids

2.5.1 Sodium hydroxide
Sodium hydroxide pellets are taken and dissolved in the water at the rate of 16 molar
concentrations. It is strongly recommended that the sodium hydroxide solution must be
prepared 24 hours prior to use and also if it exceeds 36 hours it terminate to semi solid liquid
state. So the prepared solution should be used within this time.

2.5.2 Molarity calculation

The solids must be dissolved in water to make a solution with the required concentration. The
concentration of Sodium hydroxide solution can vary in different Molar. The mass of NaOH
solids in a solution varies depending on the concentration of the solution.
For instance, NaOH solution with a concentration of 16 Molar consists of 16 x 40 = 640
grams of NaOH solids per litre of the water, were 40 is the molecular weight of NaOH. Note
that the mass of water is the major component in both the alkaline solutions.
The mass of NaOH solids was measured as 444 grams per kg of NaOH solution with a
Concentration of 16 Molar. Similarly, the mass of NaOH solids per kg of the solution for other
concentrations was measured as 10 Molar: 314 grams, 12 Molar: 361 grams, and 14 Molar:
404 grams [4].
356 R. Anuradha, V. Sreevidya, R. Venkatasubramani and B.V. Rangan

Table 3: Physical and chemical properties sodium silicate

Chemical formula Na2O x SiO2 Colour less

Na2O 15.9%
SiO2 31.4%
H2O 52.7%
Appearance Liquid (Gel)
Colour Light yellow liquid (gel)
Boiling Point 102 C for 40% acqeous solution

Molecular Weight 184.04

Specific Gravity 1.6

2.6 Experimental programme

2.6.1 Testing the concrete specimens
Twenty five 150×150mm cubes and 150mm diameter 300m high were cast out of which
three cubes each were used to determine the compressive strength and three cylinders
each were used to determine the split tensile strength at 24 hours for different grades of
Geopolymer Concrete. A total of 300 numbers of specimens were tested in this study to
find out the optimized grades of Geopolymer Concrete incorporating M-sand. Optimized
mix ratios were shown in Table 4. All geopolymer concrete were made with mix design
procedure using IS 10262-2009 [5]. It is recommended to have necessary precaution on
workers because of acidic nature of the concrete. The aggregates were prepared in
saturated-surface-dry (SSD) condition. Geopolymer concrete can be manufactured by
adopting the conventional techniques used in the manufacture of Portland cement
concrete. Then the components of concrete ingredients are collected and mixed with the
pan mixture for about 5 min. Then Alkaline liquid were then added to the mixture and the
mixing was done for another 5 min. After the mixing, the flow value of fresh geopolymer
concrete was determined in accordance with slump test IS 516-1959. The fresh concrete
could be handled up to 120 minutes without any sign of setting and without any
degradation in the compressive strength. Flow test (workability) was carried out by slump
cone test as described for cement concrete. After the flow test, fresh concrete were
placed in respected mould as described in the IS 516-1959.The fresh concrete was cast
and compacted by the usual methods used in the case of Portland cement concrete. The
specimens were left standing for 1 hour and then cured at 60ºC in the curing chamber for
about 24 hours. Demoulding was done at 24 hours at the time of curing age. After the
curing period the specimens left at the room temperature for about an hour and ready for
testing. Thus the compressive strengths and tensile strength of concrete were tested at the
same day in accordance with IS 516-1959 [6]. The reported strengths were the average of
the three specimens shown in Table 5.
 MODIFIED GUIDELINES FOR GEOPOLYMER CONCRETE... 357

Table 4: Shows the optimised mix proportions for M-sand

M1 M2 M3 M4 M5 M6
Content
kg/m3 kg/m3 kg/m3 kg/m3 kg/m3 kg/m3
Fly ash 364.9 419.7 482.6 555.0 638.2 483.7
Coarse aggregate 1049.5 1018.0 987.5 957.9 929.1 882.2
Water 36.5 44.2 44.2 44.2 44.2 14.2
NaOH solution 52.7 68.5 68.5 68.5 68.5 89.8
Na2SiO3 184.5 171.1 171.1 171.1 171.1 224.6
M-sand 613 608.1 589.9 572.2 615.6 652.1
M7 M8 M9 M 10 M 11 M12
Content
kg/m3 kg/m3 kg/m3 kg/m3 kg/m3 kg/m3

Fly ash 554.7 483.7 554.7 554.7 364.9 447.0

Coarse aggregate 832.8 882.2 832.8 832.8 964.0 907.5
Water 12.7 28.3 14.2 28.3 14.2 28.3
NaOH solution 103.0 82.2 89.8 82.2 83.0 89.8
Na2SiO3 257.5 205.5 224.6 205.5 207.3 224.6
M-sand 615.6 652.1 615.6 615.6 713 670.8

Table 5: Test results for manufactured sand

Mix Compressive strength (N/mm2) Tensile strength (N/mm2)

M1 21 1.592
M2 25 2.865
M3 22 2.865
M4 24 2.865
M5 24 2.865
M6 33 2.865
M7 20 2.4
M8 22 2.4
M9 21 2.65
M10 23 2.73
M12 20 2.73
358 R. Anuradha, V. Sreevidya, R. Venkatasubramani and B.V. Rangan

M13 21 2.865
3. DESIGN OF GEOPOLYMER CONCRETE MIXTURES

3.1 Data for mix design

The following basic data are required to be specified for design of a concrete mix:
a) Characteristic compressive strength of Geopolymer Concrete at 24 hours curing at the
temperature of 60ºC (fck).
b) Maximum size and Type of Fine aggregate and Coarse Aggregate to be used.
c) Specific gravity of ingredients of concrete.
d) Selection of Alkaline liquid, Flyash Ratio to the Compressive ratio.
Aggregates size, grading, surface texture, shape and other characteristics may produce
secretes of different compressive strength for the same tiled ratio, the relationship between
strength and free Alkaline liquid, Extra Water, Fly ash Ratio should preferably be established
for the materials [7,8,9].

3.2 Estimation of air content

Approximate amount of entrapped air to be expected in normal (non-air-entrained) concrete is
given in Table 6.
Table 6: Approximate of Air Content

Nominal maximum size of Entrapped air, as percentage of

aggregate mm volume of concrete

10 3
20 2

For the desired workability, the quantity of mixing per unit volume of concrete and the ratio
of fine aggregate to total aggregate by absolute volume are to be estimated from Tables as
applicable, depending upon the nominal maximum size and type of aggregates.

Table 7: Approximate sand per cubic metre of concrete

Sand as percentage of total

Nominal size of coarse aggregate
aggregate by absolute volume
10mm 40
20mm 35

Table 8: Adjustment of values in and sand percentage for zone factor i.e. fineness modulus

Change in condition Adjustment in sand percentage

For sand conforming to grading +1.5 percent for Zone I
Zone I, Zone III or Zone IV 0f - l.5 percent for Zone III
 MODIFIED GUIDELINES FOR GEOPOLYMER CONCRETE... 359

Table 4 of IS : 383-1970* 3.0 percent for Zone IV

3.3 Calculation of aggregate content
The total aggregate content per unit volume of concrete may be calculated from the following
equations:
 SO S F 1 Fa  1
V= + + + × and
 Sso Ss SF P SFa  1000
 SO S F 1 Ca  1
V= + + + ×
 Sso Ss SF 1 − P SC a  1000

Where,
V = Absolute volume of fresh concrete, which is equal to gross volume minus the
volume of entrapped air.
S = Sodium Silicate Solution (kg) per m3 of concrete.
SO = Sodium Hydroxide Solution (kg) per m3 of concrete
F = Weight of Flyash (kg) per of m3 of concrete
SF = Specific gravity of Flyash
P = Ratio of fine aggregate to total aggregate by absolute volume
Fa , C a = Total masses of fine aggregate and coarse aggregate (kg) per m3 of concrete
respectively
SFa , SC a = Specific gravity of saturated surface dry fine aggregate and coarse
aggregate respectively.
Ss = Specific gravity of Sodium Silicate solution.
Sso = Specific gravity of Sodium hydroxide solution.

4. ILLUSTRATIVE EXAMPLE FOR GEOPOLYMER CONCRETE MIX

DESIGN

An example illustrating the mix design for a Geopolymer concrete of M 30 grade is given
below:

4.1 Design stipulations

a) Characteristic compressive strength required at age of = 30MPa
36hours at the temperature of 60ºC
b) Maximum size of aggregate (angular) = 10mm
c) Specific gravity of fly ash = 2.3
d) Specific gravity of coarse aggregate = 2.6
e) Specific gravity of fine aggregate = 3.1
f) Sand conforming = zone III
g) Specific gravity of NaOH = 1.47
360 R. Anuradha, V. Sreevidya, R. Venkatasubramani and B.V. Rangan

h) Specific gravity of Na2Sio3 = 1.6

4.2 Solution
Step 1: Selection of fly ash to the compressive ratio

Figure 1. Shows flyash content to the compressive strength

The amount of flyash required for M30 grade =550 Kg/m3 is Derived from the above
Figure 1.

Step 2: Selection of alkaline liquid ratio

Figure 2. Generalised relation between free alkaline liquid to flyash ratio and compressive strength
of concrete

The ratio between Sodium hydroxide to sodium silicate is 1:2:5 From the table 9
The amount of alkaline liquid required accordance to compressive stress from the Figure 2.
 MODIFIED GUIDELINES FOR GEOPOLYMER CONCRETE... 361

The amount of Alkaline liquid = 0.61 x flyash content =0.61x550 = 335.5 Kg/m3
Amount of Sodium silicate Solution = 239.64 Kg/m3
Amount of Sodium Hydroxide Solution = 95.86kg/m3
Morality to be used in the concrete is 16 molar in which 444 grams of NaOH solids
dissolved in 556 grams of water. Solids = 42.56 kg/m3 Water = 53.3 kg/m3

Table 9: Sodium hydroxide to sodium silicate ratio accordance to compressive Strength

Compressive strength Sodium hydroxide Sodium silicate

10 1 3
15 1 2.5
20 1 2.5
25 1 2.5
30 1 2.5
35 1 2.5
40 1 2.5
45 1 2.5

Step 3: Selection of water content

The maximum water content to add extra is 0.06 Water to flyash ratio
The minimum water content to be added extra is 0.02 water to flyash ratio
According to workability extra water can be added this is due to flyash is arrived from
various plant which have different properties in absorption of water in order to match extra
water is added.
Amount of water add extra 0.02 to water flyash ratio = 0.03x550 = 16.5 kg/m3
362 R. Anuradha, V. Sreevidya, R. Venkatasubramani and B.V. Rangan

Figure 3. Adjustment of values in sand content percentage

Table 10: Approximate sand contents per cubic metre of concrete for grades up to M35grade

Nominal size of coarse Sand as percentage of total aggregate by

aggregate absolute volume
10mm 40
20mm 35
Change in condition Sand content in %
For sand conforming to Zone II 0%
For decrease in sand content –2.5%
Total –2.5%

From above graph decrease in sand content = 2.5%

Total aggregate by absolute volume = (40 – 2.5) = 37.5%
Estimation of Air Content

Table 11: Approximate air content

Nominal maximum size of Entrapped air as percentage of

aggregate in mm volume of concrete
10 3%
20 2%

4.3 Determination of aggregate content

From table, for the specified maximum size of aggregate of 10 mm, the amount of entrapped
air in the wet concrete is 3 %. Taking this into account and applying the following equations:
 SO S F 1 Fa  1
V= + + + × and
 Sso Ss SF P SFa  1000
 SO S F 1 Ca  1
V= + + + ×
 Sso Ss SF 1 − P SC a  1000

Where,
V = Absolute volume of fresh concrete, which is equal to gross volume minus the
volume of entrapped air.
S = Sodium Silicate Solution (kg) per m3 of concrete.
SO = Sodium Hydroxide Solution (kg) per m3 of concrete
F = Weight of Flyash (kg) per of m3 of concrete
SF = Specific gravity of Flyash
P = Ratio of fine aggregate to total aggregate by absolute volume
 MODIFIED GUIDELINES FOR GEOPOLYMER CONCRETE... 363

Fa , C a = Total masses of fine aggregate and coarse aggregate (kg) per m3 of concrete
respectively
SFa , SC a = Specific gravity of saturated surface dry fine aggregate and coarse
aggregate respectively.
Ss = Specific gravity of Sodium Silicate solution.
Sso = Specific gravity of Sodium hydroxide solution.
On substitution, in the above equation
Fine aggregate content:

0.97 = {(95.86 / 1.47 ) + (239.64 / 1.6) + (550.0 / 2.3) + (1 / (0.36 ))(Fa / 2.6) }X (1 / 1000)
Fa = 600 kg / m3
Coarse aggregate content:

0.97 = {(95.86 / 1.47 ) + (239.64 / 1.6) + (550.0 / 2.3) + (1 / (1 − 0.36))(C a / 2.6 ) }X (1 / 1000)
Fa = 838.3kg / m3

Table 12: Mix proportion

Sodium Sodium hydroxide Extra Fine Coarse

Flyash
silicate solution water aggregate aggregate
239.64kg/m3 95.86 kg/m3 11kg/m3 550 kg/m3 600 kg/m3 838.3 kg/m3
0.61 0.03 1 1.04 1.56

5. CONCLUSION

• With the generic information available on geopolymers, a rigorous trial-and-error method

was adopted to develop a process of manufacturing fly ash-based geopolymer concrete
following the technology currently used to manufacture Ordinary Portland Cement
concrete. After some failures in the beginning, the trail-and-error method yielded
successful results with regard to manufacture of low-calcium (ASTM Class F) fly ash-
based geopolymer concrete.
• Geopolymer concrete is an excellent alternative solution to the CO2 producing port land
cement concrete.
• Low-calcium fly ash-based geopolymer concrete has excellent compressive strength
within a day and is suitable for structural applications [10].
• The price of fly ash-based geopolymer concrete is estimated to be about 10 to 30
percent cheaper than that of Portland cement concrete.
• In this study it is observed that Compressive strength results obtained for M-sand was
nearly equal when compared to control concrete.
 364 R. Anuradha, V. Sreevidya, R. Venkatasubramani and B.V. Rangan

• Tensile strength of the river sand is high when compared to the M- Sand.
• Due to presence of sodium silicate as a sticky gel form in nature And also flyash is finer
element it recommended to have 20% higher than of Mix design values.
• Due to presence of sodium silicate as a gel form it take delay in setting at ambient
temperature. In order to overcome it recommended that heat curing is necessary, which
also increase the compressive Strength. The temperature to be maintained is 60ºC for
about 24hours to 48hours.

REFERENCES

1. Davidovits J. Structural characterization of geopolymeric materials with Xray

diffractometry and MAS NMR spectroscopy, Geopolymer’8: First European Conference
on Soft Mineralogy, Compiegne, France, Vol. 2, 1988, pp. 149-166.
2. Hardjito D, Rangan BV. Development and properties of low-calcium fly ash-based
geopolymer concrete, Research Report GC, Faculty of Engineering, Curtin University of
Technology, Perth, Australia, 2005, pp. 1-130.
3. IS 383-1970 Specification for coarse and fine aggregates from natural sources for
concrete.
4. Vijaya Rangan B. Mix design and production of fly ash based geopolymer concrete The
Indian Concrete Journal, May (2008)7-14.
5. IS 10262-2009 Recommended guidelines for concrete mix design.
6. IS 516 -1959 Methods of tests for strength of concrete.
7. Xu H, Lukey GC, van Deventer JSJ. The activation of class C, class F fly ash and blast
furnace slag using geopolymer, Fly ash, Silica Fume, Slag, and Natural Pozzolans in
Concrete, Proceedings Eighth International Conference, V.M. Malhotra editors, Las
Vegas, USA., 2004, pp. 797-820.
8. Fernandez J, Palomo A. Activation of fly ashes: A general view, Fly ash, Silica Fume,
Slag, and Natural Pozzolans in Concrete, Proceedings Eighth International Conference,
V.M. Malhotra editors, Las Vegas, USA, 2004, pp. 351-366.
9. Bakharev T. Durability of geopolymer materials in sodium and magnesium sulphate
solutions, Cement and Concrete Research, 35(2005) 1233-46.
10. Hardjito D, Wallah SE, Rangan BV. Study on engineering properties of fly ash-based
geopolymer concrete. Journal of the Australian Ceramic Society, No. 1, 38(2002) 44-7.

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